Blue sulfur dye and process of making same.



lUNTTEn STATES Patented December 2'7, 190%.

PATENT EETcE.

KARL ELBEL, OF BIEBRICH, GERMANY, ASSIGNOR TO THE FIRM OF KALLE ANDCOMPANY, OF BIEBRIOH, GERMANY.

BLUE SULFUR DYE AND PROCESS OF MAKING SAME.

SPECIFICATIGN forming part of Letters Patent No. 778,478, dated December27, 1904.

Application filed October 5, 1904. Serial No. 227,292.

To all 11/700711 it 'II'I/KLZ/ concern:

Be it known that I, KARL ELBEL, a subject of the King of Prussia,Emperor of Germany, residing at Biebrich, Germany, have invented certainnew and useful Improvements in the Manufacture of Blue Sulfur Dyes. ofwhich the following is a specification.

In my application for United States Letters Patent bearing the same dateI have described the mode of preparing a new monochloro-alpha-naphthol.I have now found that this monochloro-alpha-naphthol yields indophenolswhen oxidized in presence of a molecular proportion of a para diamin ofthe benzene series or of an unsymmetrical alkyl derivative of the same.These indophenols or the phenylnaphthylamin derivatives obtained byreducing the same yield valuable violet to greenish-blue sulfur colorsdyeing unmordanted cotton when heated with alkali polysulfids. I

In the following I give an example according to which thecoloring-matters may be obtained; but my invention is not limited to theproportions and other conditions mentioned therein.

Thirty-six kilos monochloro-alpha-naphthol and 27.2 kilosdimethyl-paraphenylene diamin, (OH3).1NG;HiNH2. are dissolved withtwenty-four kilos of caustic-soda lye of 40 Beaum in two thousand literswater. The solution is well cooled and mixed with a hypochloritesolution containing 29. 8 kilos NaOOl. The so-obtained indophenol isfiltered off. washed, and dissolved in about one thousand liters waterby means of one hundred kilos crystallized sodium sulfid. Theso-obtained colorless phenylnaphthylamin derivative is precipitated bythe addition of eighty-five kilos bicarbonate of soda filtered andpressed. It is then mixed with two hundred kilos sodium sullid andeighty kilos sulfur and heated gradually up to 110 centigrade.evaporizing part of the water. This temperature is maintained until thereaction is finished2 6., for about ten hours. After cooling thecoloringmatter is completely separated from the aqueous part of themelt. It may be isolated by filtration and may directly be used for dye-It may also be purified by dissolving ing.

it in a hot solution of fifty kilos sodium sulfid in one thousand litersof water by filtering the solution and by reprecipitating thecoloring-matter by means of a current of air or by the addition ofcommon salt.

The thus-produced dyestuff is a dark-blue powder insoluble in water,soluble in alcohol with blue color, easily soluble in water in presenceof sodium sulfid and dyeing unmordanted cotton from such a solution fastgreenish-indigo shades.

IVhat I claim is 1. The manufacture of violet to greenishblue sulfurdyes by heating with alkali polysulfids the indophenols orphenylnaphthylamin derivatives obtained by simultaneous oxidation ofmonochloro-alpha-naphthol and of a paradiamin of the benzene series.

2. The manufacture of a blue sulfur dye by simultaneous oxidation ofmonochloro-alphanaphthol and dimethyl-paraphenylenediamin (OHQNOGHINHQand by heating the so-obtained indophenol directly or after transformingit into the colorless phenylnaphthylamin derivative with alkalipolysulfid.

3. The new sulfur dyes obtained by heating with alkali polysulfids theindophenols or phenylnaphthylamin derivatives produced by simultaneousoxidation of monochloro-alphanaphthol and a paradiamin of the benzeneseries, which are dark-blue powders insoluble or very little soluble inwater, easily soluble in an aqueous sodium-sulfid solution and dyeingfrom such solutions violet to greenish-blue shades on unmordantedcotton.

4:. The new blue sulfur dye obtained from monochloro-alphanaphthol anddimethylparaphenylenediamin substantially as described which is adark-blue powder insoluble in water, soluble in alcohol with blue color,easily soluble in water in presence of sodium sulfid and dyeingunmordanted cotton from such a solution fast greenish-indigo shades.

In testimony whereof I have signed my name to this specification in thepresence of two subscribing Witnesses.

KARL ELBEL.

I/Vitnesses:

IGNAZ ROSENBERG, J EAN GRUND.

